US10760180B2 - Polycrystalline silicon ingot, polycrystalline silicon bar, and method for producing single crystal silicon - Google Patents
Polycrystalline silicon ingot, polycrystalline silicon bar, and method for producing single crystal silicon Download PDFInfo
- Publication number
- US10760180B2 US10760180B2 US15/785,895 US201715785895A US10760180B2 US 10760180 B2 US10760180 B2 US 10760180B2 US 201715785895 A US201715785895 A US 201715785895A US 10760180 B2 US10760180 B2 US 10760180B2
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- United States
- Prior art keywords
- polycrystalline silicon
- temperature
- single crystal
- minute
- producing single
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 82
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 25
- 238000002844 melting Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims description 47
- 230000008021 deposition Effects 0.000 claims description 9
- 229910021419 crystalline silicon Inorganic materials 0.000 claims 6
- 239000013078 crystal Substances 0.000 description 42
- 230000008034 disappearance Effects 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 10
- 239000010703 silicon Substances 0.000 description 10
- 238000000151 deposition Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/34—Single-crystal growth by zone-melting; Refining by zone-melting characterised by the seed, e.g. by its crystallographic orientation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
Definitions
- the present invention relates to polycrystalline silicon ingots and polycrystalline silicon rods suitable for stably producing single crystal silicon.
- Single crystal silicon essential for production of devices such as semiconductor devices is grown by the CZ method or the FZ method, and a polycrystalline silicon ingot or a polycrystalline silicon rod is used as the raw material in such a case.
- a polycrystalline silicon material is produced, in many cases, by the Siemens method.
- the Siemens method is a method in which a gas of a silane raw material such as trichlorosilane or memosilane is brought into contact with a heated silicon core wire to thereby allow polycrystalline silicon to grow in the vapor phase (deposit) on the surface of the silicon core wire by the Chemical Vapor Deposition (CVD) method.
- CVD Chemical Vapor Deposition
- a polycrystalline silicon ingot is placed in a quartz crucible and heated to be melted, a seed crystal is dipped in the resulting silicon melt to extinguish dislocation lines to achieve freedom from dislocation, the crystal diameter is being slowly increased until the diameter of the crystal reaches a predetermined diameter, and then the crystal is pulled up.
- the unmelted polycrystalline silicon remains in the silicon melt, the unmelted polycrystalline pieces drift in the vicinity of the solid-liquid interface by convection to induce the generation of dislocation, and thus the polycrystalline silicon remaining unmelted causes the crystal line to disappear.
- inhomogeneous crystals which are needle crystals, may be deposited during a process of producing a polycrystalline silicon rod by the Siemens method; if single crystal silicon is grown by the FZ method using the polycrystalline silicon rod in which the needle crystals have been deposited, individual crystallites are not melted homogeneously according to their sizes because of the aforementioned inhomogeneous crystals; and then, the unmelted crystallites as solid particles pass through the melting zone toward the single-crystal rod and are incorporated as unmelted particles into the solidified surface of the single-crystal, thereby causing disappearance of crystal lines.
- the present invention has been made in view of such problems and aims to provide a polycrystalline silicon ingot and a polycrystalline silicon rod suitable for stably producing single crystal silicon.
- a polycrystalline silicon ingot according to the present invention is characteristic of having a value of T e ⁇ T s , ⁇ T, of 50° C. or less, wherein T s and T e are the onset temperature and the completion temperature of melting, respectively, when the temperature is increased at a rate of 60° C./minute or less in the temperature range of 1400° C. or more.
- the polycrystalline silicon ingot is a polycrystalline silicon ingot extracted from a polycrystalline silicon rod synthesized by the Siemens method.
- the polycrystalline silicon rod according to the present invention is a polycrystalline silicon rod synthesized by the Siemens method and characterized in that a polycrystalline silicon ingot extracted from any portion of the polycrystalline silicon rod has a value of T e ⁇ T s , ⁇ T, of 50° C. or less, wherein T s and T e are the onset temperature and the completion temperature of melting, respectively, when the temperature is increased at a rate of 60° C./minute or less in the temperature range of 1400° C. or more.
- the polycrystalline silicon ingot or polycrystalline silicon rod aforementioned is used as the raw material for production of single crystal silicon by the CZ method and the FZ method.
- the polycrystalline silicon ingot according to the present invention which exhibits the melting property described above, markedly prevents disappearance of crystal lines when a single crystal silicon is produced.
- polycrystalline silicon ingots and polycrystalline silicon rods suitable for stably production of single crystal silicon are provided.
- single crystal silicon is grown by the CZ method
- polycrystalline silicon is melted in a crucible, and then, a seed crystal silicon rod is immersed in the silicon melt and drawn up while rotated to obtain a single crystal ingot having the same atomic arrangement as that of the seed crystal.
- a seed crystal is placed under the polycrystalline silicon rod. The seed crystal and the polycrystalline silicon rod are melted at their boundary by induction heating, and this silicon melt is single-crystallized while held by surface tension.
- the present inventors thus have conducted heating and temperature-increasing tests on polycrystalline silicon raw material in which disappearance of crystal lines was caused and polycrystalline silicon raw material in which disappearance of crystal lines was not caused, to thereby observe melting phenomena in the temperature increasing process and compare the melting properties.
- cylindrical cores having a diameter of 19 mm were gouged from each portion of a polycrystalline silicon rod grown by the Siemens method. From these cores, planar samples having a thickness of 2 mm were cut out, and the surface of the samples were mirror-finished by buffing.
- Such a planar sample was placed in an alumina container and heated using a halogen lamp at a rate of temperature increase of 50° C./minute at room temperature (25° C.) to 200° C., of 200° C./minute at 200° C. to 1200° C., and of 50° C./minute at 1200° C. to 1500° C.
- the rate of temperature increase in a temperature range of 1200° C. to 1500° C., which includes the melting point of silicon is 60° C./minute or less, observation is not hindered.
- the atmosphere in the measurement environment was a reducing atmosphere of argon containing 2% hydrogen gas.
- the melting point of silicon which is of the order of 1414° C., exceeds 1000° C. At such a high temperature, a large amount of infrared light is emitted not only from the sample itself but also from the surroundings of the sample. Thus, it is not possible to observe the state of the melting sample by the naked eye or with an optical microscope. Then, only a limited region at a small depth of focus (observation face was 4 mm ⁇ 2 mm) was observed using a laser microscope, which allows an observation without effects of infrared light. As the laser microscope, a VL 2000 manufactured by Lasertec Corporation was used, and as the light source, a blue laser diode (wavelength 410 nm) was used.
- An image having a resolution of 0.15 ⁇ m and a magnification of 560 was video-recorded.
- the temperature of the sample surface was measured with a thermocouple thermometer provided at the lower part of the alumina container aforementioned, and the temperature was recorded in synchronization with the sample image. While the image reproduced was observed, the temperature at the moment of the beginning of melting (T s ) and the temperature at the moment where the entire mass was melted (T e ) were measured.
- the present inventors consider that a deposition rate of 5 ⁇ m/minute or more is preferred in order to synthesize polycrystalline silicon that satisfies the melting conditions aforementioned by the Siemens method. According to the experience of the present inventors, when polycrystalline silicon grown under conditions that produce polycrystalline silicon at a low deposition rate is melted, “unmelt” tends to remain in the melt.
- the value of T e ⁇ T s , ⁇ T, described above is constant at a rate of temperature increase of 60° C./minute or less.
- a smaller ⁇ T value is shown with a higher rate of temperature increase. This is because the temperature at the moment of the beginning of melting (T s ) and the temperature at the moment where the entire mass was melted (T e ) become difficult to distinguish when the rate of temperature increase is extremely high.
- the rate of temperature increase is preferably 60° C./minute or less.
- Example 1 Example 2 Disappearance Rate of temperature increase (° C./minute) of crystal lines 50 60 70 80 A1 Not observed T s (° C.) 1,475 1,470 1,465 1,4760 T e (° C.) 1,500 1,495 1,485 1,475 ⁇ T e ⁇ T s (° C.) 25 25 20 15 A2 Not observed T s (° C.) 1,450 1,450 1,440 1,435 T e (° C.) 1,500 1,500 1,480 1,470 ⁇ T e ⁇ T s (° C.) 50 50 40 35 B1 Observed T s (° C.) 1,440 1,435 1,430 1,425 T e (° C.) 1,500 1,495 1,485 1,475 ⁇ T e ⁇ T s (° C.) 60 60 55 50 B2 Observed T s (° C.) 1,430 1,425 1,420 1,415 T e (° C.) 1,500 1,495 1,495 1,495 1,495 1,495
- polycrystalline silicon rods grown under different deposition conditions were provided. These polycrystalline silicon rods, which were grown by the Siemens method, were deposited by varying the growth rate (deposition rate) in the range of 2 to 10 ⁇ m/minute with the concentration of trichlorosilane, which is the silicon raw material gas, held constant at 30 vol %.
- the single crystal silicon ingot according to the present invention which exhibits the melting property described above, markedly prevents disappearance of crystal lines when the single crystal silicon is produced.
- polycrystalline silicon ingots and polycrystalline silicon rods suitable for stably production of single crystal silicon are provided.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2016-204077 | 2016-10-18 | ||
| JP2016204077A JP2018065710A (ja) | 2016-10-18 | 2016-10-18 | 多結晶シリコン塊、多結晶シリコン棒、および単結晶シリコンの製造方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| US20180105950A1 US20180105950A1 (en) | 2018-04-19 |
| US10760180B2 true US10760180B2 (en) | 2020-09-01 |
Family
ID=61765024
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US15/785,895 Active US10760180B2 (en) | 2016-10-18 | 2017-10-17 | Polycrystalline silicon ingot, polycrystalline silicon bar, and method for producing single crystal silicon |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US10760180B2 (de) |
| JP (1) | JP2018065710A (de) |
| CN (1) | CN107954427B (de) |
| DE (1) | DE102017009638A1 (de) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020125242A (ja) * | 2020-06-01 | 2020-08-20 | 信越化学工業株式会社 | 多結晶シリコン塊、多結晶シリコン棒、および単結晶シリコンの製造方法 |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4123989A (en) * | 1977-09-12 | 1978-11-07 | Mobil Tyco Solar Energy Corp. | Manufacture of silicon on the inside of a tube |
| JPS61127617A (ja) | 1984-10-30 | 1986-06-14 | ロ−ヌ−プ−ラン・スペシアリテ・シミ−ク | 超高純度シリコン棒の製造方法 |
| JPH03215310A (ja) | 1990-01-19 | 1991-09-20 | Osaka Titanium Co Ltd | 多結晶シリコンの製造方法 |
| US20080286550A1 (en) | 2007-05-16 | 2008-11-20 | Wacker Chemie Ag | Polycrystalline Silicon Rod For Zone Reflecting And A Process For The Production Thereof |
| US20120251426A1 (en) * | 2009-12-14 | 2012-10-04 | Jx Nippon Mining & Metals Corporation | Polycrystalline Silicon For Solar Cell And Preparation Method Thereof |
| JP2012232878A (ja) | 2011-05-09 | 2012-11-29 | Shin-Etsu Chemical Co Ltd | シリコン芯線ホルダおよび多結晶シリコンの製造方法 |
| JP2012232879A (ja) | 2011-05-09 | 2012-11-29 | Shin-Etsu Chemical Co Ltd | シリコン芯線ホルダおよび多結晶シリコンの製造方法 |
| JP2013193902A (ja) | 2012-03-16 | 2013-09-30 | Tokuyama Corp | 多結晶シリコンロッド |
| JP2016052970A (ja) | 2014-09-04 | 2016-04-14 | 信越化学工業株式会社 | 多結晶シリコン製造用反応炉、多結晶シリコン製造装置、多結晶シリコンの製造方法、及び、多結晶シリコン棒または多結晶シリコン塊 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010040587A (ja) * | 2008-07-31 | 2010-02-18 | Covalent Materials Corp | シリコンウェーハの製造方法 |
-
2016
- 2016-10-18 JP JP2016204077A patent/JP2018065710A/ja active Pending
-
2017
- 2017-10-16 CN CN201710958219.6A patent/CN107954427B/zh active Active
- 2017-10-17 US US15/785,895 patent/US10760180B2/en active Active
- 2017-10-17 DE DE102017009638.4A patent/DE102017009638A1/de active Pending
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4123989A (en) * | 1977-09-12 | 1978-11-07 | Mobil Tyco Solar Energy Corp. | Manufacture of silicon on the inside of a tube |
| JPS61127617A (ja) | 1984-10-30 | 1986-06-14 | ロ−ヌ−プ−ラン・スペシアリテ・シミ−ク | 超高純度シリコン棒の製造方法 |
| US4734297A (en) | 1984-10-30 | 1988-03-29 | Rhone-Poulenc Specialites Chimiques | Production of shaped articles of ultra-pure silicon |
| JPH03215310A (ja) | 1990-01-19 | 1991-09-20 | Osaka Titanium Co Ltd | 多結晶シリコンの製造方法 |
| US20080286550A1 (en) | 2007-05-16 | 2008-11-20 | Wacker Chemie Ag | Polycrystalline Silicon Rod For Zone Reflecting And A Process For The Production Thereof |
| JP2008285403A (ja) | 2007-05-16 | 2008-11-27 | Wacker Chemie Ag | 帯域引き上げ用の多結晶シリコンロッド及びその製造方法 |
| US20120251426A1 (en) * | 2009-12-14 | 2012-10-04 | Jx Nippon Mining & Metals Corporation | Polycrystalline Silicon For Solar Cell And Preparation Method Thereof |
| JP2012232878A (ja) | 2011-05-09 | 2012-11-29 | Shin-Etsu Chemical Co Ltd | シリコン芯線ホルダおよび多結晶シリコンの製造方法 |
| JP2012232879A (ja) | 2011-05-09 | 2012-11-29 | Shin-Etsu Chemical Co Ltd | シリコン芯線ホルダおよび多結晶シリコンの製造方法 |
| US20140030440A1 (en) * | 2011-05-09 | 2014-01-30 | Shin-Etsu Chemical Co., Ltd. | Silicon core wire holder and polycrystalline silicon manufacturing method |
| JP2013193902A (ja) | 2012-03-16 | 2013-09-30 | Tokuyama Corp | 多結晶シリコンロッド |
| US20150107508A1 (en) | 2012-03-16 | 2015-04-23 | Tokuyama Corporation | Polycrystalline Silicon Rod |
| JP2016052970A (ja) | 2014-09-04 | 2016-04-14 | 信越化学工業株式会社 | 多結晶シリコン製造用反応炉、多結晶シリコン製造装置、多結晶シリコンの製造方法、及び、多結晶シリコン棒または多結晶シリコン塊 |
| US20170225957A1 (en) | 2014-09-04 | 2017-08-10 | Shin-Etsu Chemical Co., Ltd. | Reaction furnace for producing polycrystalline silicon, apparatus for producing polycrystalline silicon, method for producing polycrystalline silicon, and polycrystalline silicon rod or polycrystalline silicon ingot |
Non-Patent Citations (1)
| Title |
|---|
| Office Action dated Aug. 13, 2019, issued in counterpart JP Application No. 2016-204077, with English translation (8 pages). |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2018065710A (ja) | 2018-04-26 |
| US20180105950A1 (en) | 2018-04-19 |
| CN107954427A (zh) | 2018-04-24 |
| CN107954427B (zh) | 2022-11-01 |
| DE102017009638A1 (de) | 2018-04-19 |
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